• The Korean Journal of Pesticide Science
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• v.19 no.2
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• pp.81-87
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• 2015

The present study was aimed to predict the pre-harvest residue limits (PHRLs) of pyrimethanil (fungicide) and methoxyfenozide (insecticide) in grape, and to estimate their biological half-lives and residual characteristics. The pesticides were sprayed once on grape in two different fields 10 days before harvest. At the end of 0, 1, 2, 3, 5, 7 and 10 days after application, samples were harvested for further analysis. The residual pesticides were extracted with acetonitrile and partitioned with dichloromethane, and the high-performance liquid chromatography with diode array detector (HPLC/DAD) was employed for the residue analysis. The results obtained in the present study show that the limit of detection of both pesticides were found to be $0.01mg\;kg^{-1}$. The recoveries of these pesticides were ranged between 80.6% and 102.5% with coefficient of variation lower than 10%. The biological half-lives of both pesticides were observed in field 1 and field 2 which shows 7.7 and 7.4 days for pyrimethanil and 5.1 and 6.1 days for methoxyfenozide, respectively. Further, the PHRL of pyrimethanil and methoxyfenozide was found to be $8.90mg\;kg^{-1}$ and $5.51mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggests that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when grape is harvested.

• The Korean Journal of Pesticide Science
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• v.20 no.4
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• pp.319-325
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• 2016

This study was conducted to investigate residual organochlorine pesticides in green house soil and oriental melon, green pepper, and lettuce. The majority of them were designated as persistent organic pollutants (POPs) by the international community at the Stockholm Convention on Persistent Organic Pollutant. Extraction and clean-up method were developed using the QuEChERS method for residual organochlorine pesticides (OCPs) in soil and oriental melon, green pepper and lettuce. Recovery of OCPs in greenhouse soil and oriental melon, green pepper, and lettuce ranged from 73.3-110.6%. Limit of detection (LOD) of OCPs in soil and 3 crops were 0.01-0.08 and $0.11-0.17{\mu}g/kg$. The residues of OCPs in oriental melon, green pepper and lettuce greenhouse soil were analyzed by the developed method, and dieldrin, ${\beta}-endosulfan$ and endosulfan sulfate were detected at 1.4-72.5, 0.1-78.7 and $0.0-214.1{\mu}g/kg$, respectively. The detection frequency of 3 compounds in soils were 52 (29.7%), 34 (19.4%) and 57 (32.6%) among 175 samples, respectively. However, these compounds were not detected in all crop samples. The residue level in 3 crops were lower than 1/58.8 of maximum residue level of them. These results showed that the OCPs residue in oriental melon, green pepper, and lettuce greenhouse soil were not as high as crop safety threatening.

• Journal of Food Hygiene and Safety
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• v.31 no.2
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• pp.85-93
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• 2016

A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

• Journal of Food Hygiene and Safety
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• v.32 no.1
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• pp.35-41
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• 2017

To determine the contents of sodium and potassium in side dishes, 92 samples from 22 different kinds of side dishes that can be classified into 3 groups were collected in Seoul area and analysed using ICP-OES. The highest sodium content was detected in pepper doenjang muchim, while potassium content was the highest in kong jorim. When comparing the content of sodium and potassium in 3 groups, namely namul, muchim, and jorim, the sodium content of namul group was significantly different from those of jorim and muchim (p-value < 0.05). Sodium intake per serving size was the highest in parae muchim among the samples as estimated to 20.2% of WHO recommendation that is 2,000 mg/day. The amount of sodium by simultaneously intake of soybean sprouts namul, anchovy jorim and parae muchim per one serving size was estimated to 1,000 mg. The potassim/sodium ratios of spinach namul and kong jorim were 1.70 and 0.81, respectively, while that of bracken namul was very low as about 0.1. Food-borne pathogens were not detected out of 92 side dishes.

• Analytical Science and Technology
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• v.28 no.5
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• pp.323-330
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• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Korean Chemical Engineering Research
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• v.49 no.2
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• pp.168-174
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• 2011

Various La-based perovskite catalysts were prepared by a Pechini method, and they were applied to the low-temperature oxidation of odor compounds exhausted from waste food treatment process for effective deodorization. Quantitative and qualitative analyses of exhausted gas were conducted to measure the amount of major odor compounds with respect to operation time. A standard odor sample composed of major odor compounds was then prepared for use as a feed for oxidation reaction system. Various transition metal(M)-substituted La-based perovskite catalysts ($LaMO_{3}$: M=Cr, Mn, Fe, Co, and Ni) were prepared and applied to the oxidation of odor compounds in order to investigate the $LaNiO_3$ catalyst showed the best catalytic performance. Pt-substituted perovskite catalysts ($LaNi_{1-x}Pt_{x}O_{3}$: x=0, 0.03, 0.1, and 0.3) were then prepared for enhancing the catalytic performance. It was found that $LaNi_{0.9}Pt_{0.1}O_{3}$ catalyst served as the most efficient catalyst. Supported perovskite catalysts ($XLaNi_{0.9}Pt_{0.1}O_{3}/Al_{2}O_{3}$: X=perovskite content(wt%), 0, 10, 20, 30, 40, 50, and 100) were finally applied for the purpose of maximizing the catalytic performance of perovskite catalyst in the low-temperature oxidation reaction. Catalytic performance of $XLaNi_{0.9}Pt_{0.1}O_{3}/Al_{2}O_{3}$ catalysts showed a volcano-shaped curve with respect to perovskite content. Among the catalysts tested, $20LaNi_{0.9}Pt_{0.1}O_{3}$/$Al_{2}O_{3}$ catalyst exhibited the highest conversion of odor compounds of 88.7% at $180^{\circ}C$.

• Horticultural Science & Technology
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• v.33 no.4
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• pp.591-597
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• 2015

We determined the total C and N stocks in trees and soils after 1 year of fertilization in an experimental orchard with 16-year-old 'Niitaka' pear (Pyrus pyrifolia Nakai cv. Niitaka) trees planted at $5.0m{\times}3.0m$ spacing on a Tatura trellis system. Pear trees were fertilized at the rate of 200 kg N, 130 kg P and $180kg\;K\;ha^{-1}$. At the sampling time (August 2013), trees were uprooted, separated into six fractions [trunk, main branches, lateral branches (including shoots), leaves, fruit, and roots] and analyzed for their total C and N concentrations and dry masses. Soil samples were collected from 0 to 0.6 m in 0.1 m intervals at 0.5 m from the trunk, air-dried, passed through a 2-mm sieve, and analyzed for total C and N concentrations. Undisturbed soil core samples were also taken to determine the bulk density. Dry mass per tree was 5.6 kg for trunk, 12.0 kg f or m ain branches, 15.7 kg for lateral branches, 5.7 kg for leaves, 9.8 kg for fruits, and 10.5 kg for roots. Total amounts of C and N per tree were respectively 2.6 and 0.02 kg for trunk, 5.5 and 0.04 kg for main branches, 7.2 and 0.07 kg for lateral branches, 2.6 and 0.11 kg for leaves, 4.0 and 0.03 kg for fruit, and 4.8 and 0.05 kg for roots. Carbon and N stocks stored in the soil per hectare were 155.7 and 14.0 Mg, respectively, while those contained in pear trees were 17.8 and $0.2Mg{\cdot}ha^{-1}$ based on a tree density of 667 trees/ha. Overall, C and N stocks per hectare stored in the pear orchard were 173.6 and 14.2 Mg, respectively. Compared with results obtained in 2012, the amounts of C stocks have increased by $17.7Mg{\cdot}ha^{-1}$, while those of N stocks remained virtually unchanged ($0.66Mg{\cdot}ha^{-1}$).

• Korean Journal of Soil Science and Fertilizer
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• v.37 no.4
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• pp.212-219
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• 2004

To minimize the danger of soil erosion and settle habitats earlier, afforestation, which vegetates bare slopes, is selected as an environmental recovering technology. Large portions of these areas often are suffered by a bad germination and growth inhibition of sprayed seeds. Afforested materials collected in the normal and damaged sites were not any big difference in chemical characteristics and biological response to ryegrass. But background soil of the damaged site has very low pH (3.6) and high contents of iron and aluminum compared with them of the normal sites. Both germination and root growth of ryegrass were inhibited severely in the water extracts of damaged soils, but not in the water extracts of normal sites. Groundwater collected nearby the damaged sites was very strong acidic (pH 33) and exhibited a high value of electrical conductivity and high contents of iron and aluminum. In the ground water, germinated ryegrass was scarcely grown. In Al standard solution, the root growth of ryegrass was inhibited over 50% in 0.5 mM in pH 3.5-4.5 and in 1.4 mM in pH 5.5, which seems to be related to $Al^{3+}$ activity in solution. In the ferric Fe ($Fe^{3+}$) standard solution, ryegrass growth was inhibited over 50% in the concentration of 14-19 mM in root and 23-25 mM in shoot. This strong tolerance of ryegrass to $Fe^{3+}$ might be concerned with the very low activity of $Fe^{3+}$ at pH 3.5-5.5. In contrast, ryegrass responded very sensitively to ferrous Fe ion ($Fe^{2+}$), especially in root growth: $Fe^{2+}$ concentrations corresponding to 50% growth reduction were 0.3-0.4 mM at pH 3.5-5.5 in roots. This high growth inhibition should be related to the high ion activity of $Fe^{2+}$ irrespective of different pH conditions. In conclusion, low pH and high contents of $Fe^{2+}$ and aluminum seem to be caused by pyrite and be closely related to the growth inhibition of ryegrass seeded in afforested area.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.8
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• pp.1165-1170
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• 2010

A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.343-349
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• 2012

Exposure and risk assessments were conducted to evaluate the relative safety of mixing/loading work of indoxacarb between wettable powder (WP) and water dispersible granule (WG). Hand exposure was monitored using cotton gloves while inhalation exposure was measured using personal air monitor. Method validation for the exposure monitoring was established successfully through several experiments. Limit of determination and limit of quantitation were 0.25 and 1 ng, respectively. $R^2$ of calibration curve linearity was more than 0.9999 and reproducibility was 0.7-6. Recovery of indoxacarb from gloves, solid sorbent and glass fiber filter at three different levels was 81.5-108.8%. Trapping efficiency and breakthrough tests gave 981.5-108.8% of recovery. During mixing/loading procedure, hand exposure amount (75 percentile of 30 repetitions) for indoxacarb WP was 6 folds (459.8 mg/kg a.i) than that of WG (81.4 mg/kg a.i). This result indicates that WG has less drift than WP thanks to its granular type of formulation. Inhalation amount was $10^{-8}-10^{-7}%$ of spray mixture prepared and $10^{-4}-10^{-3}%$ of hand exposure. In inhalation case, no significant differences were observed between two formulations. Margin of safety was calculated for risk assessment using male Korean average body weight and acceptable operator exposure level as the important exposure factors. Mixing/loading procedures for both of the formulations were considered to be of least risk because calculated MOS values were more than 1.